A copy of the presentation I delivered in September 2015 as part of my Final Year Project for the Master of Professional Engineering (Mechanical) at the University of Western Australia.
Please note: This was simply uploaded after the presentation was delivered as an example to friends studying engineering and what to expect in a final year presentation. Therefore, it lacks the full explanation required to understand the project in significant detail. Further information is available by contacting me directly.
This research furthered the development of micro-electro-mechanical sensors for use in recycled water monitoring and lab-on-a-chip medical devices. AlGaN/GaN sensors are superior to traditional ion-selective field effect transistor sensors because the are more stable, cost less and do not require a reference electrode.
Completing this project involved using the Australian Synchrotron to measure the molecular contact angle of three molecules, glycine, 6-amino-2-naphthoic acid in benzil, on the surface of an AlGaN/GaN high electron mobility transistor-based chemical sensor. The project was able to determine the angle for two out of the three chemicals used, which was a great success given the experimental difficulty of conducting near-edge x-ray absorption fine structure spectroscopy.
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Surface Chemistry and Device Response of AlGaN/GaN Sensors
1. Surface Chemistry and Device Response
on AlGaN/GaN surfaces
Jeremy Gillbanks – September 2015
Supervised by
Prof. Giacinta Parish and Prof. Brett Nener
2. Sensor Context
1
Semiconductor
Doping
High Electron Mobility
Transistors
Substrate Design
Field Effect
Transistors
Chemical Sensors
Chemical
Sensors
Field Effect
Transistors
CHEMFETs ISFETs
Silicon-based
devices
Heterostructure-
based devices
HEMTs
AlGaN/GaN AlGaAs/GaAs
BioFETs
Other
Sensors
3. Our Sensors
2
Semiconductor
Doping
High Electron Mobility
Transistors
Substrate Design
Field Effect
Transistors
Chemical Sensors
Chemical
Sensors
Field Effect
Transistors
CHEMFETs ISFETs
Silicon-based
devices
Heterostructure-
based devices
HEMTs
AlGaN/GaN AlGaAs/GaAs
BioFETs
Other
Sensors
4. AlGaN/GaN Sensors
Advantages over traditional
ISFET Sensors
– Stability
– Low cost
– No reference electrode
Applications
– Recycled water
monitoring
– Lab-on-a-chip sensor
arrays
3
AlGaN capped transistor
Ren 2008
Sensor array design
Asadnia 2015
Active area
5. Research Gap
Previous research completed by the Microelectronics
Research Group at UWA
4
Demonstrating ionic
concentration,
regardless of pH
(2010)
Dipolar molecule
orientation and
sensor response
Sensor selectivity
toward negative ions
(2010)
GaN cap has greater
affinity to Cl- ions than
AlGaN (2014)
2DEG conductivity
increase with positive
charge build up
(2014)
6. Project Objectives
Aim: Molecular contact angle vs. device response
5
Glycine
Benzil (non-polar)
6-Amino-2-Naphthoic Acid
Hypothesis:
• Adhesion via negatively
charged carboxyl group
• Dipolar molecules will affect
device response via molecular
orientation
This is the first time dipolar molecular orientation has been
investigated on a GaN capped device.
7. Molecule Selection
Glycine 6-Amino-2-Naphthoic Acid
NEXAFS conducted at AS
C N
Background Correction
Choose Step Edge
Gaussian Peak Fitting
Spectral Subtraction
Bond Angle Calculation
Molecular Orientation
Compare to Device Response
O
Benzil
Experimental Procedure
6
6-Amino-2-Naphthoic Acid only
8. Molecule Selection
Glycine 6-Amino-2-Naphthoic Acid
NEXAFS conducted at AS
C N
Background Correction
Choose Step Edge
Gaussian Peak Fitting
Spectral Subtraction
Bond Angle Calculation
Molecular Orientation
Compare to Device Response
O
Benzil
Project Scope
7
6-Amino-2-Naphthoic Acid only
9. Molecule Selection
Glycine 6-Amino-2-Naphthoic Acid
NEXAFS conducted at AS
C N
Background Correction
Choose Step Edge
Gaussian Peak Fitting
Spectral Subtraction
Bond Angle Calculation
Molecular Orientation
Compare to Device Response
O
Benzil
Seminar Scope
8
6-Amino-2-Naphthoic Acid only
10. NEXAFS: How it works
• Near Edge X-ray Absorption Fine Structure
9
• Incident photon energy is
near the edge of the
ionisation potential of the
scanned atom
• Ammeter allows
replacement current to be
recorded from
photoelectron loss
• Allows measurement of
individual molecular orbitals
for C, N and O atoms
Experimental Setup
Mennell 2015
This is the first time a NEXAFS study has been conducted
on a GaN substrate
15. Identifying the peak
14
Measured angle from nitrogen scan: 43.7˚ ± 10˚
Measured angle from carbon scan: 46˚ ± 2˚ (Home 2015)
Naphthoic Acid Peak fit at 404 eV (corresponds to C-N σ* bond)
16. Angle of naphthoic acid
to surface
I can corroborate Michael Home’s finding that 6-
amino-2-naphthoic acid lies at 44˚ to the device
surface.
15
44˚
Device Surface
17. Future Work
• Ensure adequate coverage
• Normalise on the device surface
• Test simple alcohols/acids
– Methanol
– Formic acid
– Benzoic acid
• Test simple amine groups
– Methylamine
– Aniline
• Test simple amino acids with
benzene rings
– Meta-, ortho-, or para-amino
benzoic acid
• Later: test larger molecules
– Tyrosine
16
Tyrosine
Formic acid Aniline
18. Key Points
• We have been the first to successfully orientate
glycine and 6-amino-2-naphthoic acid on a GaN
capped device
– Every molecule to be sensed has a specific angle at
which it adheres to the surface
– The orientation effects the device response
• Future work has been successfully identified
• Special thanks to
– Prof. Giacinta Parish & Prof. Brett Nener
– Farah Khir, Matt Myers, Murray Baker
– Michael Home, Chris Mennell, Ben Sutton
– The III-N research group
17
20. Background Correction
• Remove oscillations in
incident photon intensity
over time and energy
• Au leaf used (300 eV –
1000 eV)
19
Device setup at the Australian Synchrotron
Courtesy: F. Khir
23. Sources of Error & Biases (1/2)
• Noise
– Using peak areas instead of peak heights decreases
effect of noise on local regression
• Local regression formula inadequately smoothed
• Back scattered electrons
– Reduced to insignificance due to multiple incident angles
– Highly energetic photons (with adequate coverage)
shouldn’t penetrate the adsorbate
• Photoelectrons generated from surrounding atoms
• Thermal motion ineffectively averaged between scans
22
24. … (2/2)
• Monochromator’s linearly polarised light
– K-shell spectra are highly polarisation-dependent
– Linear polarisation simplifies the dipole matrix element
• Replacement current efficiency (resistance, etc…)
• Inconsistent incident photon intensity in excess of what is
corrected for using the reference foil
• Substrate does not display three-fold or higher symmetry
• Adsorbate not a homogenous layer
• Hydrogen bonds effect spectra in a measurable way
• Ineffective spectral subtraction
• Adsorbate damaged during x-ray scan
23
25. Limitations
• Building block model
– Used when you have a new molecule that has not
been scanned using NEXAFS before
• E.g. 6-amino-2-naphthoic acid or benzil
– Limitations:
• Conjugated molecular orbitals are difficult to identify
during deconvolution
• More of a problem for carbon K-edge NEXAFS scans
24
26. Why not more samples?
• AS has high resolution
– Resolution: 0.1 eV
– Energy Range: ~40 eV
– 0.25% steps
• Trends successfully identified => conclusions are
valid
• Common practice is to use best spectra, not to
average
• Experiment cost: ~$600k
25
27. References
1. Title Slide:
Substratehttp://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.
svc/ImageService/Articleimage/2006/DT/b515727g/b515727g-f5.gif
2. Title Slide: Australian Synchrotron logo
https://events.synchrotron.org.au/event/1/picture/10.jpg
3. Title Slide: Microelectronics Research Group
http://mrg.ee.uwa.edu.au/images/microelectonicsResearchGrou.gif
4. Slide 5: Glycine
http://www.actgene.com/images/Glycine.jpg
5. Slide 5: 6-Amino-2-Naphthoic Acid
http://www.sigmaaldrich.com/content/dam/sigma-
aldrich/structure6/165/mfcd01861831.eps/_jcr_content/renditions/mfcd01861831-medium.png
6. Slide 5: Benzil
http://www.sigmaaldrich.com/content/dam/sigma-
aldrich/structure3/116/mfcd00003080.eps/_jcr_content/renditions/mfcd00003080-medium.png
7. Slide 15: 6-Amino-2-Naphthoic Acid
http://pubchem.ncbi.nlm.nih.gov/image/img3d.cgi?cid=2733954
8. Slide 16: Formic Acid
http://chem-tracking.de/onewebstatic/ed4ba8c401-Ameisensäure.jpg
9. Slide 16: Aniline
http://chemwiki.ucdavis.edu/@api/deki/files/9113/aniline.png
10. Slide 16: Tyrosine
http://img1.wikia.nocookie.net/__cb20140401122944/resscientiae/images/2/29/Tyrosine.jpg
All other slides are of the author’s creation unless otherwise cited.
26
Editor's Notes
Stability: less drift & non-toxic, even at high power applications or hostile conditions (pH, temperatures, etc…)
Low cost: uses current MOSFET (common) manufacturing methods
No ref. electrode: smaller sizes => sensor arrays
Applications: recycled water monitoring, air pollution monitoring, biomonitoring (anything that’s real-time)
Lab on a chip sensor arrays (each sensor can be individually functionalised to detect a particular ion or molecule)
Sensor selectivity: negative end of molecules sticks to surface
GaN cap: better due to better affinity to ions
Ionic concentration: suitable for use in an array of sensors
2DEG concentration: changes with molecules impacting the surface
Unknown: dipolar molecule orientation and how it impacts sensor response
Include reasons for molecules
Explain Synchrotron
Explain how NEXAFS works
Why the inner shell electrons? Why not the outer ones? – The outer ones vary to widely. Inner ones detail atomic structure.
Mention what it is physically
Why it is important
Identify it on the graph
Mention where is must be
Near the ionisation potential
Or at least near to it
Explain why there may be a difference (physisorbed)
How wide the initial guess must be from literature
How high the guess must be
Why choose Gaussian peaks
How to guess initial locations based on physical bonds
How to guess heights/widths based on LOESS operation
How it works (assumptions)
Limitations of building block method
N-scan
Ga XPS
Get substrate spectral locations
Subtract from 6A2NA
Identify final peak
Identify angle
Get substrate spectral locations
Subtract from 6A2NA
How the peak was chosen
Why peak areas rather than peak height?
With noisy signal data (like ours) smoothing is required to fit a local regression fit
Smoothing distorts the signal and peak height
=> Use peak area where smoothing is not required
0.3% different from literature value
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